Papers by Keyword: Calcium Phosphate Cement (CPC)

Abstract: In this work properties of potential brushite (CaHPO4•2H2O) and hydroxyapatite (Ca10(PO4)6(OH)2) compound cements are investigated. Calcium dihydrogenphosphate monohydrate (MCPM) and α-tricalcium phosphate (α-TCP) were the starting materials for investigated cements. Setting time is controlled by adding setting time retarder – citrate ions and initially unreactive filler - monetite (CaHPO4). Some compositions of obtained cements contain both brushite and hydroxyapatite. However a substantial amount of monetite was present even if it is not added as filler. There is a strong evidence of presence of octacalcium phosphate – a precursor phase for hydroxyapatite that lacks long range order.

Abstract: An injectable calcium phosphate cement (CPC) modified with sodium citrate was developed in the present study. The effects of sodium citrate concentration on the injectability, mechanical strength, and the self-setting properties of CPC were systematically investigated. The addition of sodium citrate significantly improved injectability and compressive strength of CPC. The specimens have an injectability of 93% and compressive strength of 36.43 ± 2.64 MPa at 15 wt% sodium citrate concentration, compared to injectability of 75% and compressive strength of 23.15 ± 2.12 MPa of the specimens without sodium citrate. XRD spectra indicated that addition of sodium citrate did not change the hydration reaction of CPC and the reaction product was mainly poorly crystallized hydroxyapatite. In conclusion, CPC developed in this work exhibited excellent injectability and high strength, which should be a promising material for bone repair.

Abstract: To improve the physicochemical properties of calcium phosphate cement (CPC), silk fibroin (SF) in the different forms were added into CPC. The structure of the composites was studied by X-ray diffraction. The setting time was investigated by ISO Cement Standard Consistency Instrument. Scanning Electron Microscope was used to observe the surface morphology. Mechanical properties of samples were tested by Instron Universal Testing Machine. The results indicated that acicular crystal of hydroxyapatite (HA) was formed in the hardening body of both CPC with SF and the pure CPC. Addition of SF had no significant effect on the structure of SF/CPC composite. The setting time of CPC with SF was significantly shorter than that of the pure CPC (30.3 mins). The setting time of CPC by adding silk fibroin powder I (SFP) and silk fibroin fiber (SFF) was greatly shortened, which was only 11.7 minutes. The setting time of CPC with SFP decreased approximately by 1/3, while the setting time of the CPC with SFF decreased nearly by 1/2. With the adding of SF, the compressive strength of CPC increased significantly. There was a distinct increase in the work-of-compressive of CPC with the adding of SFF.

Abstract: The objective of this study is to compare the degradation of three strontium-containing calcium phosphate cement (Sr-CPC) and one calcium phosphate cement without strontium (CPC) in vivo. Three Sr-CPCs, containing 1%, 5%, 10% strontium respectively, and a CPC without strontium were tested in this study. The specimens in rod-shape (2 mm  6 mm) were prepared, and were implanted in the erector spine muscle of 15 New Zealand rabbits. After 4, 8 and 12 weeks, 5 rabbits were sacrificed respectively and the specimens were taken out, cleaned, dryed and weighed. The weight losses of the specimens were calculated and the data were analyzed by ANOVA. The results showed that the CPC containing 5%, 10% strontium showed obviously higher degradation rates at the three observation periods than that containing 1% strontium and that without strontium (P<0.05). Addition of 1% strontium into CPC did not increase degradation rate (P>0.05), and the CPC containing 5% and 10% strontium showed no difference in degradation rate at the three observation periods (P>0.05).

Abstract: A new class of osteoconductive and osteoinductive combination biomaterials composed of calcium phosphate cement (CPC), demineralized bone matrix (DBM) and a water-soluble viscosity modifier were prepared and characterized in-vitro and in-vivo. In previous studies, a range of combinations formulations were tested in order to compare their performance characteristic. In-vitro characterization results show that the mechanical strength is decreased when the amount of DBM increases. However, DBM does not affect the CPC’s ability to set hard and convert to nanocrystalline apatitic calcium phosphate, which shares the chemical structure of natural bone as seen in x-ray diffraction. It is known that the DBM alone is osteoinductive. In-vivo osteoinductivity testing of the formulations in an intramuscular, athymic rat model demonstrated that the combination material is also osteoinductive. Two formulations were chosen for in-vivo efficacy testing based on the results of in-vitro and in-vivo characterization. These formulations were studied using rabbit critical-sized femoral core defect model. The formulations were composed of DBM with particle sizes of 250 to 710 μm, carboxymethyl-cellulose (CMC) as the viscosity modifier and weight percent compositions of 50% DBM/ 45% CPC/ 5% CMC and 60% DBM/ 30% CPC/ 10% CMC. Bone integration and healing was graded at 6, 12, and 24 weeks. The two formulations were compared to the gold standard autograft at 12 weeks and to an empty defect as the negative control at 24 weeks. Based on micro-computed topography (μCT), both formulations allowed for continuity of bone throughout the defect region at all time points. No differences in dense area fraction were seen between two formulations at 6 weeks (p = 0.8661). There was no significant statistical difference between the two formulations and autograft at 12 weeks (p = 0.2467). At 24 weeks, both formulations had significantly higher dense area fractions than empty controls (p = 0.0001). Histologically, the biology of the treatment areas appeared to have returned to normal by 24 weeks with CPC appearing to be the principal osteogenic inducer. In conclusion, these combinations of CPC and DBM offers significant advantages (handling, mechanical properties and osteoinductivity) over current DBM products and can be an effective alternative to autograft in healing of bone defects.

Abstract: Alpha-bsm® is a first generation self-setting, injectable and moldable apatitic calcium phosphate cement (CPC) based on amorphous calcium phosphate (ACP). ACP was prepared using low temperature double decomposition technique, from a calcium solution (0.16 M), and phosphate solution (0.26 M) in a basic (pH~13) media. ACP was than stabilized using three crystal growth inhibitors (CO32-, Mg2+, P2O74-), freeze-dried, and heated (450 °C, 1h) to remove additional moisture and some inhibitors. Dicalcium phosphate dehydrate (DCPD) was also prepared using wet chemistry at room temperature from calcium and phosphate solution, respectively, 0.3 M and 0.15 M. ACP and DCPD powder were combined at a 1:1 ratio and ground to produce Alpha-bsm® bone cement. The cement is supplied as a powder and when mixed with an appropriate amount (0.8 ml/g) of physiological saline at room temperature, forms an injectable putty-like paste. The paste has a working time of about 45 minutes at room temperature, when stored in a moist environment. The setting reaction proceeds isothermically at body temperature (37°C) in less than 20 minutes, forming a hardened, porous (total porosity 50 to 60%), low crystalline (40% comparing with HA), apatitic calcium phosphate cement with a compressive strength range of 10 to 12 MPa. Extensive pre-clinical studies (rabbit radius critical sized defect, canine tibia osteotomy, sheep tibia, primate fibula fracture healing, and primate fibula critical size defect) demonstrate that Alpha-bsm® undergoes remodeling in conjunction with new bone formation. The next generation of Bone Substitute Materials (Beta-bsmTM and Gamma-bsm TM) are formulated based on the Alpha-bsm® chemistry but differ in powder processing (e.g. milling) technique. These materials are also self-setting, injectable and/or moldable apatitic calcium phosphate cements with improved handling and mechanical properties. The setting & hardening reaction of these new CPCs proceeds isothermically in less than 5 minutes at 37°C and once hardened demonstrate a compressive strength of 30 to 50 MPa. The final product (after full conversion) is a low crystalline (40% compared with Hydroxyapatite), calcium deficient (Ca/P atomic ratio = 1.45) carbonated apatite similar to the composition and structure of natural bone mineral (crystal size: length = 26 nm, width thickness = 8 nm). A desirable feature of these cements is their high surface chemistry (with specific surface area of about 180-200 m2/g) which is ideal for remodeling and controlled release of growth factors. A pilot rabbit critically sized femoral defect study comparing the three synthetic family products demonstrate that they share similar remodeling and resorption characteristics up to 52 weeks. Physico-chemical and mechanical performance of these next generation CPCs are favorable when compared with existing CPCs in the market, specifically material working time (at room temperature), cohesivity in a wet environment and fast setting & hardening rate (at body temperature).

Abstract: In the present study, three types of tetracalcium phosphate (TTCP) were prepared by solid-solid reaction or co-precipitation method and by different cooling modes. The effect of TTCP on the performance of calcium phosphate cement (CPC) was investigated. The result showed that the characteristic of TTCP varied with preparation method and played an important role in CPC performance. A solid-solid reacted TTCP yielded smaller particle size and resulted in bad workability and mechanical strength of CPC. The fast cooling of sintering TTCP by liquid nitrogen could avoid the decomposition of TTCP and make pure TTCP. TTCP prepared by wet-precipitation could improve performance of CPC and was promising to optimization of CPC.

Abstract: Exothermal behavior is always present during the hydration of cements. The biocompatibility and curing effect of a bone cement is in close relationship with its exothermal behavior. The exothermal behavior in the hydration process of the partially crystallized calcium phosphate (PCCP)+dicalcium phosphate anhydrate (DCPA) system cement was studied in this article. The results show that with the decrease of the particle size of DCPA, the heat release rate was greatly increased; whereas, with the decrease of the particle size of PCCP, the heat release rate was not obviously altered. The heat release in the hydration process of the PCCP+DCPA system cement was only 137 J/g, which was quite smaller than that of the tetracalcium phosphate (TTCP)+dicalcium phosphate dihydrate (DPCD) system cement, and the temperature increase was very small for this cement.

Abstract: Three dimensional printing was investigated for fabricating hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) composite scaffolds using calcium phosphate based ceramics and calcium phosphate cement chemistry. Scaffolds were formed by printing an aqueous sodium phosphate solution on the powder bed consisting of a mixture of dicalcium phosphate anhydrous (DCPA) and calcium hydroxide powders. The sodium phosphate solution was functioning as a binder material and also as the initiator of the wet chemical reaction. Compressive mechanical properties of printed samples were examined as a function of saturation level that was inversely proportional to the powder to liquid ratio. To increase mechanical properties and obtain hydroxyapatite and β-TCP composites, the printed samples were sintered. The effect of sintering parameters including dwell time and sintering temperature were also examined. X-ray diffraction (XRD) was used to examine material composition at different stages of the manufacturing process and to confirm the presence of HA and β-TCP in the final stage. The effect of sintering procedure on the surface topology of the samples was examined using scanning electron microscopy (SEM).

Abstract: Single-component, self-setting and injectable calcium phosphate cement (CPC) based on amorphization process of dicalcium phosphate dehydrate (DCPD) is proposed. After preparation of DCPD by wet chemistry, the material was dry milled in an Attritor high energy process (at 400 RPM) during 20 minutes. Experiments were also conducted using a regular ball milling process at 15 and 30h residence time. Amorphization of DCPD confirmed using FTIR, XRD and 31 P solid-states NMR (cross-polarization and decoupling). Upon hydration of amorphized DCPD powder with saline (0.55 ml/g), putty-like consistency produced. The paste hardened in 30 minutes at 37°C and reached a compressive strength of about 20 MPa. The final product was a low crystalline calcium deficient apatite, similar to the composition and structure of bone mineral.